Process of preparing manure.



JOHANN HAMMERSCHLAG, OF. STRASSBURG, GERMANY.

' PROCESS OF PREPARING MA NURE.

Specification of 'Letters Patent.

Patented Dec. 11, 1906.

Application filed October 15, 1902. Serial No. 127,426.

Be it known that I, JOHANN HAMMER- SCHLAG, director, a subject of the King of Prussia, German Emperor, residing at Strassburg, Alsace, in the Empire of Germany, have invented new and useful Improvements in Processes of Preparing Manures, of which the following is a specification.

This invention relates toimprovements in the manufacture of fertilizers and artificial manures; and it is intended to devise means for converting and keeping the fertilizing constituents of such compounds in a soluble state and for preventing their reversion, by which means the fertilizing and plant-nourishing value of the compound is increased and they are converted into a state which allows of their easy adaptability and of their bein stored for any length of time and of being siipped without damage.

The rather sli ht solubility of the fertilizer compounds ren ers their action very unreliable if it is intended to make them available for the next crop. For this reason manufacturers have been tr 'ng to convert the valuable constituents o the raw materials which enter into the composition of the fertilizers into soluble or easily-available compounds,

' .While at the same time avoiding to render the 'mlc aci our in SOll are capable of dissolvm s1l1c1c final product strongly acid or alkaline, inasmuch as fertilizers exhibitin such decided reactions, and in particular t ose having an kalies and suitable salts and minerals, such.

as phos hates, silicates, and the like; Huand its allied substances which ocacid and-its salts on being submitte tothe treatment about to be described and t undergo decom ositions whereby compounds are formed w 'ch retain their. solubility for any length of time. The same'eflect is produced by the treatment with humic acid of phosphates in (place of or in combination with silicic acid an its salts. Both the solutions of humic acid as well as the solutions of the compounds of the 'humic acid with silicic acid or with its salts are also capable of dissolving natural phosphates, whereby the valuable fertilizing agents are rendered available and made soluble and converted into a st ate in which they will be easily absorbed by the plants.

Where Imake mention of humic acid in the specification this term includes the putrefied decayed vegetable or animal matters which result from the slow decomposition of animal, and in particular vegetable, material and Which are soluble in water with the addition of alkalies or ammonia, such matters occurring in large quantities in brown coal, lignite, peat-bog, forest earth, humus, and the like. The term humic acid as used in the specification is to include also those substances which are designated as humine acid, ulmic acid, -ulmine, gcic acid,

kreine acid, kreic acid, kreine, apokreine acid, and allied substances which are obtained from the above-mentioned materials or which are intermediate "products of decomposition. Also soot which is the product of dry distillation of carboniferous material yields, if treated in the same manner as decayed or putr'efied vegetable or animal materials, a solution of humic acid. Humic acid may also be obtained by treatment of carbon with acids, and with nitric acid in particular. I p

The prgparation of the solution of humic acid is e e above-mentioned materials or a mixture of any of the same with a cold or hot a ueous solution of caustic alkali, (KOH,NaO am- 'monia, (NH or with the corres onding carbonates of the same (K 00 a CO (NHQ QO' in a suitable manner by pressure, ifnecessary, the materials having been mixed to the consistency of a paste. Peat, bog, forest earth, lignite, soot, or other substances rich in carbon are suitable for the purpose. The above-mentioned alkaline solutlons may cted by treating any one of the be re laced by other substances containing free. a kali and not interferin otherwise with the action of fertilizers. bus I may use, for instance, the s0- called. soluble glass for effecting the solution. By this treatment the major part of the carbomferous material is changed so asto become soluble in water. The thus-obtained soluble humie acid may be poured off, filtered, or squeezed out, and

p sists of humicacid. For every one I (56.16:40.06=17: m; :c=,12.1.)

- which'the "tries beyond the-sea,-

suited for the purpose.

the resultant liquid may then be evaporated and dried. It 1s immaterial for the fertilizing action whether they soluble constituents are admixed in the form of a aste or as a dry powder or combined with msoluble substances.

As an instance of carrying my invention into effect, I may.mention the followin rela tive roportions of materials which I have foun to be suitable for most purposes. Thus I may use one hundred parts of marsh earth containing about twenty-five per cent. of solid matter, of which latter one-half conhundred parts of dry humic acid I may use seventeen parts of caustic potash, (K,()H.) Instead of potash I may use equivalent proportions of other alkaliesthus' for instance, of caustic soda, 12.1 parts of caustic soda corresponding to seventeen parts of" caustic potash,

These proportions can of course be somewhat varied, according to the properties of the material submitted to the treatment. The right proportions will always have to be found out by experiments in each articular case, and the amount of water to e used will alsohave to be ascertained by experiments. I'n'the above instance I have found a proportion of one thousand parts of water for every two hundred and fifty parts of dry bog'to bebest This treatment of the above enumeratedmaterials,

same by. means of alkaline li uids, the extraction of the humic acid by d ssolution, the

1 separation of the liquid'by filtration, squeezmg ofi, evaporating, drying, and pulverizing constitutes the first step of the process for the.

im roved fertilizer or artificial -manure in manufacture of a fertilizer in accordance their solubility, the product presenting the further advantage ofpreserving its physical condition, even on being stored for a long time and after having been shipped to counso that 1t will not acquire a hard and stone-like appearance, but retains the valuable properties of fertilizers in general-that is to-'sa the roperty of being easily strewn an 1 distri uted and spread, upon which property its adaptability for many purposes-will chiefly depend. The further treatment of the compound thus ob-- tained is efiectedby intimately mixing the.

. humic-acid solution produced either in form of a filtrate or'in admixture with the undissolved -rendere rtion of the bog 8 available with-silicates and com-' which are rich in carbon, the rendering available of the and very valuable properties soluble and dissolved components are contained in such a state as to retainwhich has been pounds or mixtures of which silicates form a part. These materials are employed in a finely-powdered condition, the mixture or the dissolving being effected either cold or at an elevated temperature and, if required, under'pressure.

A suitable quantity of water has to be present, such as is required for the dissolving of the newly-formed combination of the silicates with, humic acid, for which purpose the amount of water present in the process of converting the humic acid will generally be sufficient. After the decomposition and the solution has been finished, which sometimes 1 may take several days, the solution is squeezed out, evaporated, and dried, or the entire mass containing a mixture of dissolved and undissolved material is dried, powdered,

and sifted. In this case also the amount of silicates or silicic acid to be'added will depend on various circumstances. In the above-mentioned example I have found thirty parts, by weight, of-silicate of potash as an addition to one hundred parts, by

4 weight, of the-solids of converted humic-acid,

which solids are to be computed from the go abovementioned data, to be suitable for the purpose.

\ I In manufacturing this fertilizing material the-use of silicates of alkalis, silicate of potash, silicate of sodium, sol ble glass will 5 chiefly suggest itself; but ti' varying the working conditions accordinly as regards degree or heat, pressure, and duration of treatment other silicious material-such as infusorial earth or kieselguhr, which are morereadily attacked'may be used;

After the solution of the silicates the new compound which the silicates have formed with the humic acid retains its easy solubility even onprolonged drying. The silicates are 10 5 thereby converted into entirely new compounds, which are made up of materials rich in carbon, such as peat, and which are rendered available by treatment with alkali and of silicates, .and the new compounds also con- 1 1c tain humous silicic-acid? compounds and are exceedingly valuable .on account oi, their easy and last solubility. This will appear from the to lowing statement: 1 Upon precipitating the siliclc acid of asilicate in solution by means of acids and then submitting the precipitate toa prolonged dryin process the silicic acid becomes insoluble,- w e thenew compound obtained in the manner above described, and which contains dissolved humic 12o.

acid and dissolved silicic acid, u on being precipitated lay acids leaves a resi ue,which 1s\al ways reail acid has been change into a newcorn ound. S1l1c1c acid is sometimes used-ass ertilizmg material-in form of. silicates. It willeven y and comdpletely soluble in water even upon prolongs drying at a high temperature, which roves at the silicic become available; but its adaptability is diminished by the facts that the silicates of alkali frequently, evenafter a short time already, become hard as a rock and insoluble and form lumps and stone-hard masses, and they are thus changed into a state where their availability becomes impossible by their physical condition. I All these inconveniences are overcome by the valuable properties of the new product as above set forth.

By the above-mentioned solution of humic acid also natural phosphates may be converted and rendered soluble, as I have found by experiment. For this purpose powdered phosphatessuch as Thomas flour, powdered Thomas slag, guano, phosphorit, bone meal, bone ash, and the likeare mixed with the strongly-concentrated alkaline solution of humic acid ,as above described, in the proportion of one part, by weight, of phosphate and two parts, by weight, of humate, and the mixture is then allowed to stand for some time in the cold or at an elevated temperature and, if desired, under pressure. A decomposition will now take place, by which the phosphate is rendered available.

As a further instance of carrying out my invention I may mention the following: Fresh bog earth containing about twenty-five per cent. of dry substance is mixed with an amount of caustic alkali equal to seventeen per cent. of said dry substance and which is dissolved in thirty-four parts of water. The mixture is rubbed up with the addition of further small quantities of water, so as to lorm a thin paste. The converted humic acid is thus rendered soluble. The solution which is separated from the remaining solids is evaporated to syrupy consistence and ismixed with one-third of phosphate, for instance, -with powdered Thomas slag, by

which means a stiff jelly-like mass is formed,

which solidifies after having been kept for several days at an elevated temperature. By then adding water, stirring up, separating from the insoluble and evaporating the solution, crystals of a phosphor-humic-acid com- ]pound are obtained. This compound will e manufactured on a large scale only as an exce tion for the purpose of manufacturing ferti izers; but this decomposition is effected directly with the already-treated materials which are rich in carbon and with the phosphates, and the, product obtained is used for fertilizing purposes. The above-mentioned example, however, will be illustrative of the fact that the decomposition takes place. This manner of treatment will also prevent the already-available phosphoric acid to become insoluble a ain or to be reverted, as itisusually calle The powderedphosphates may also be mixed with the solution of compounds of the humic and silicic acid and may form fertilizing materials which contain humie acid, silicic acid, and phosphoric acid at the same time and in a readily-absorbablo state. i

Wherever it should be required to suit certain conditions and for obtaining certain results, the following materials may also be incorporated with the mass: Carbonate of magnesia, silicate of magnesia, crude and purified silicate 'of potash, magnesia and sulfite of magnesia, kainite, karnalite, sulfates, nitrates, and phosphates of alkalis and. of ammonia, and of the alkaline earth, apatit, silicate of ammonia, soluble phosphates, such as superphosphate, double superphosphate, available raw phosphates, guano, bone-meal, and the like, animal refuse, such as hair, horn, blood, powdered meat, and the like.

The fertilizing materials manufactured in the manner above described are easily soluble and assimilable A great proportion of the ingredients for nourishing the plant has already been converted into the state of humus during the dissolving and mixing process, while another partis converted while the material is kept in store up to the final conversion into the finished product, whereby the objectionablestrong caustic properties become obliterated in the very mild humicacid combination rich in carbon. For this reason such fertilizing materials may be applied at any time with a perfect reliability .evcn upon very delicate plants by strewing, spreading, pouring, and the like. If saltpeter, for instance, is used as a fertilizing material, the permissible quantity of the substance is comparately small, inasmuchas a larger quantity would destroy the roots of the plants; but if saltp'eter is employed in mixture with the solution of humic acid six times as much of saltpeter may be used with the humic acid for the same surface of soil to be treated without any harm being done to the roots of the plants. By this means valuable and cheap fertilizing materials in large quantities may be used on the plants, whereby the fertilizing action of the artificial manure is still further increased.

What I claim as my invention, and desire States, is

1. The process of manufacturing a fertilizer which consists in treating humine with solutions of'alkaline metal bases, addingsilicates of alkali and phosphates, and drying and comminuting the product, substantially as described.

2. The rocess of manufacturing a fertilizer, whic consists in treating humine with solutions of'alkaline metal bases at an ele- I vated tem erature, adding silicates of alkali to secure by Letters Patent of the United be made available by these means so as to 6 i and hosp ates, and dryin and comminut- 1 ing t e product, substantia y as described.

3. The recess of manufacturing a ferti- In witness whereof I have hereunto si ned l1zer, wh1c consists in treating humine with my name in the presence of two subscri ing solutions-0f alkaline metal bases at an elewitnesses.

vated temperature and under pressure, add- JOHANN HAMMERSOHLAG. 5 ing silicates of alkali and phosphates, and dry- Witnesses:

ing and comminuting the final product, sub GUSTAV Senwmss,

stantially as described. MARTHA L. BRITTAIN. 

